CN109279626B - Nano-sheet potassium ion battery positive electrode material, preparation method thereof and potassium ion battery - Google Patents
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Abstract
The invention discloses a nano-flake potassium ion battery anode material, a preparation method thereof and a potassium ion battery, wherein the molecular formula of the nano-flake potassium ion battery anode material is K2CuxZn1‑x[Fe(CN)6]Wherein x is more than or equal to 0 and less than or equal to 1; the preparation method of the nano flaky potassium ion battery positive electrode material comprises the following steps: dissolving potassium ferrocyanide in a deionized water solution to obtain a solution A; dissolving soluble copper salt and soluble zinc salt in an alcohol solution, and heating and stirring to obtain a solution B; dropwise adding the solution B into the solution A, and carrying out precipitation reaction under the assistance of ultrasonic waves to obtain a precipitation product; washing and drying the precipitate to obtain the nano flaky potassium ion battery anode material, wherein the preparation method is simple, the preparation period is short, and the prepared material can be used without other treatment processes; preparation of K2CuxZn1‑x[Fe(CN)6]The crystallinity is good; the nano-sheet effectively shortens the transmission path of potassium ions, so that the assembled potassium ion battery has higher first coulombic efficiency and long cycle life.
Description
Technical Field
The invention relates to a nano-sheet potassium ion battery positive electrode material, a preparation method thereof and a potassium ion battery, and belongs to the technical field of energy conversion materials.
Background
At present, with the large consumption of non-renewable energy sources such as coal, petroleum and the like, energy crisis and environmental problems caused by the consumption of the non-renewable energy sources force people to continuously explore novel energy sources, and clean renewable energy sources such as wind energy, solar energy, tidal energy and the like become important substitutes for sustainable energy development. However, due to the intermittent and random characteristics of renewable energy sources, the energy supply fluctuation is large, and high-efficiency energy storage technology is matched with the energy supply fluctuation to realize energy storage and stable output, and electrochemical energy storage with the advantages of high efficiency, stability and the like is the most ideal energy storage technology at present. Among various energy storage technologies, lithium ion batteries have a large share in the electrochemical energy storage market at the present stage due to the characteristics of high energy conversion efficiency, convenient use, long cycle life and the like. However, with the wide application of large-scale energy storage and electric vehicles, lithium ion batteries as main power sources are facing the dilemma of lithium resource shortage and increasing cost. The development of a novel secondary battery technology with no resource limitation and high energy density is a key direction for breaking through the dilemma. Sodium and lithium belong to the same main group, have similar chemical properties, and are abundant and widely distributed in nature, so that the sodium-ion battery is expected to meet the application requirement of large-scale energy storage. However, the energy density and power density of sodium ion batteries are still difficult to replace lithium ion batteries due to the large radius of sodium ions and the high standard electrode potential. The potassium which belongs to the alkali metal element also has similar physicochemical properties, and has abundant resource reserves which are close to sodium and are more than 1000 times of the lithium reserves, and the cost is only one ninth of the lithium. Meanwhile, the standard electrode potentials of lithium, sodium and potassium in the organic electrolyte are-2.88V lower than-2.79V of lithium and-2.56V of sodium, and the lower potential is favorable for improving the energy density of the battery. Compared with lithium ions and sodium ions, potassium ions have higher ionic conductivity in organic electrolyte, and higher power characteristics are favorably obtained. In addition, researches show that the rate of potassium ion insertion and diffusion in the carbon negative electrode material is faster than that of sodium ion, so that the rate capability is more excellent. Therefore, the potassium ion battery is a new energy storage battery system which is very worthy of attention based on the advantages.
The research on potassium ion batteries is still in the beginning stage, and electrode materials which can be applied to the potassium ion batteries are continuously explored. Particularly, in the case of a positive electrode material as a "potassium source", whether potassium ions can be reversibly intercalated into and deintercalated from the material is a major problem in the research of potassium ion batteries. Researches prove that the Prussian blue and the analogues thereof have an open three-dimensional tunnel structure, so that potassium ions can be reversibly deintercalated in crystal lattices of the Prussian blue, and the Prussian blue is one of the most suitable positive electrode materials of the potassium ion battery. Is stable like other de-intercalation materialsThe electrochemical reaction of the ion-doped prussian blue material depends on the matching of the size of the de-intercalation ions and the ion diffusion channel, and potassium ions can be perfectly matched with the lattice structure of the potassium ions in the prussian blue material, so that long-acting stable reversible de-intercalation is realized. However, the electrochemical performance of the prussian blue compound is greatly influenced by the crystallinity of the material, and a certain amount of structural water exists in the prussian blue compound in the general preparation process, and the structural water occupies the position of potassium ions to influence the battery capacity, and the structural water blocks the migration of the potassium ions in the crystal structure to influence the rate capability. If the structural water can be effectively reduced, the reversible specific capacity, the cycle life and the rate capability of the structural water can be further improved, so that a suitable preparation method needs to be explored urgently. In addition to the effects of structural water, diffusion of solid potassium ions is an important consideration, requiring control of the material microstructure, e.g., Fe (CN)6]When the particle size is 1-2 um, the reversible specific capacity is 53.8 mAh/g, and when the particle size is reduced to 50-75 nm, the reversible specific capacity can be as high as 121.4 mAh/g. Obviously, the proper morphology is also an important aspect for improving the electrochemical performance. The development of the cathode material with good crystallinity and proper microstructure and the preparation method thereof have very important practical significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a nano flaky potassium ion battery anode material which has good crystallinity, a proper microstructure and good potassium ion mobility, and the potassium ion battery prepared by the nano flaky potassium ion battery anode material has high coulombic efficiency for the first time, high reversible specific capacity and good cycling stability.
In order to solve the technical problems, the technical scheme of the invention is as follows: a nanometer flaky potassium ion battery anode material with a molecular formula of K2CuxZn1-x[Fe(CN)6]Wherein x is more than or equal to 0 and less than or equal to 1.
Furthermore, the thickness of the lamella of the positive electrode material of the nano flaky potassium ion battery is 20-40 nm.
The invention also provides a preparation method of the nano flaky potassium ion battery positive electrode material, which comprises the following steps:
s1: dissolving potassium ferrocyanide in a deionized water solution to obtain a solution A;
s2: dissolving soluble copper salt and soluble zinc salt in an alcohol solution, and heating and stirring to obtain a solution B;
s3: dropwise adding the solution B into the solution A, and carrying out precipitation reaction under the assistance of ultrasonic waves to obtain a precipitation product;
s4: and washing and drying the precipitate to obtain the nano flaky potassium ion battery anode material.
Further, in step S2, the soluble copper salt is any one of copper nitrate, copper sulfate, copper acetate, and copper chloride; and/or the soluble zinc salt is any one of zinc nitrate, zinc sulfate, zinc chloride and zinc acetylacetonate; and/or in step S2, the alcohol solution is one or a mixture of at least two of ethylene glycol, 1, 2-propylene glycol and glycerol.
Further, in step S2, the heating temperature during heating and stirring is 45 to 75 ℃.
Further, in step S2, the total concentration of the soluble copper salt and the soluble zinc salt in the solution B is 0.1-0.5 mol/L.
Further, in step S3, the dropping rate of the solution B is 1.0 to 5 ml/h.
Further, in step S3, the power of the ultrasonic wave is 400-800W, and the frequency is 40 KHz.
Further, in step S3, the temperature change of the reaction solution caused by the ultrasonic wave should be controlled by using circulating water, and the temperature range is 25-35 ℃.
Further, in step S3, the volume ratio of solution A to solution B is (1.05-2): 1.
The invention also provides a potassium ion battery which is made of the nano flaky potassium ion battery anode material.
After the technical scheme is adopted, the invention has the following beneficial effects:
(1) the invention provides a novel potassiumPositive electrode material K of ion battery2CuxZn1-x[Fe(CN)6]The lithium ion battery has an open three-dimensional tunnel structure, reversible storage and rapid de-intercalation of potassium ions can be realized at the gap position in the structure, the lithium ion battery is suitable for the potassium ion battery of organic electrolyte, the reversible specific capacity is 70.2 mAh/g, and the first coulombic efficiency is as high as 93.5%;
(2) k prepared by the invention2CuxZn1-x[Fe(CN)6]The material has good crystallinity, the microstructure is a monodisperse nano-layered structure, the thickness of a lamellar layer is small, the migration distance of potassium ions and electrons can be effectively shortened, meanwhile, the contact area of the lamellar structure with electrolyte is enlarged, the volume change in the de-intercalation process is relieved, and therefore good cycle performance is obtained.
(3) The preparation method provided by the invention has the advantages of simple process, high production efficiency, low requirement on required equipment, no need of other treatment processes after preparation, low energy consumption and suitability for large-scale industrial production.
Drawings
FIG. 1 shows K in example 12Cu[Fe(CN)6]An XRD pattern of the material;
FIG. 2 shows K in example 12Cu[Fe(CN)6]SEM images of the material;
FIG. 3 shows K in example 22Cu0.6Zn0.4[Fe(CN)6]SEM images of the material;
FIG. 4 shows K in example 22Cu0.6Zn0.4[Fe(CN)6]A TEM image of the material;
FIG. 5 shows K in example 22Cu0.6Zn0.4[Fe(CN)6]The charge-discharge curve of the material is 2.0-4.0V and 10 mA/g;
FIG. 6 shows K in example 22Cu[Fe(CN)6]The cycle performance curve of the material;
FIG. 7 shows K in example 32Zn[Fe(CN)6]SEM image of material.
Detailed Description
In order that the present invention may be more readily and clearly understood, a more particular description of the invention briefly described above will be rendered by reference to specific embodiments that are illustrated in the appended drawings.
Example 1:
the molecular formula of the nano flaky potassium ion battery positive electrode material of the embodiment is K2Cu[Fe(CN)6]The specific preparation method comprises the following steps:
s1: dissolving potassium ferrocyanide in deionized water solution with the concentration of 0.6 mol/L, placing the solution in an ultrasonic generating device, and taking water as a propagation medium;
s2: dissolving copper acetate into ethylene glycol solution at 55 ℃, wherein the concentration is 0.4 mol/L;
s3: dropwise adding a copper acetate alcohol solution into a potassium ferrocyanide aqueous solution at the speed of 2.5 ml/h by using an injection pump, carrying out a precipitation reaction, simultaneously loading ultrasonic waves with the power of 550W, replacing medium water in an ultrasonic device by using circulating water in order to adjust the reaction temperature rise caused by loading the ultrasonic waves, and controlling the reaction temperature to be about 30 ℃; the volume ratio of the final copper acetate alcohol solution to the potassium ferrocyanide aqueous solution is 1: 1.05;
s4: and washing and drying the obtained precipitate to obtain a material, thus obtaining a final finished product.
Phase analysis was performed on the material obtained in example 1 by X-ray diffraction (XRD) using a Rigaku TTR-lll X-ray diffractometer with a 2 θ scan ranging from 10 to 70 °, as shown in fig. 1, with high diffraction peak intensity and sharp peak shape, indicating that the prepared material has good crystallinity, and compared to standard PDF cards, the prepared material has a typical prussian blue cubic structure (JCPDS number 51-1897); the morphology of the finished product was observed by Scanning Electron Microscopy (SEM) using Hitachi X-650 as an instrument, as shown in FIG. 2, the material exhibited a monodisperse, nano-platelet structure with varying sizes.
Example 2:
the molecular formula of the nano-sheet potassium ion battery positive electrode material provided by the embodiment is K2Cu0.6Zn0.4[Fe(CN)6]The preparation method comprises the following specific steps: (
S1: dissolving potassium ferrocyanide in deionized water solution with the concentration of 0.4 mol/L, placing the solution in an ultrasonic generating device, and taking water as a propagation medium;
s2: dissolving copper acetate and zinc nitrate into ethylene glycol solution at 55 ℃, wherein the total concentration of metal ions is 0.2 mol/L;
s3: dropwise adding the mixed alcohol solution into a potassium ferrocyanide aqueous solution at the speed of 2 ml/h by using an injection pump, carrying out precipitation reaction, simultaneously loading ultrasonic waves with the power of 600W, replacing medium water in an ultrasonic device by using circulating water in order to adjust the reaction temperature rise caused by loading the ultrasonic waves, and controlling the reaction temperature to be about 30 ℃; the volume ratio of the final copper acetate alcohol solution to the potassium ferrocyanide aqueous solution is 1: 1.1;
s4: and washing and drying the obtained precipitate to obtain a material, thus obtaining a final finished product.
Scanning Electron microscope on K prepared in example 22Cu0.6Zn0.4[Fe(CN)6]The microstructure study was carried out on a material using the same equipment as in example 1, which likewise showed a monodisperse nano-platelet structure with a single thickness of about 25nm, as shown in FIG. 3; meanwhile, through further observation by a transmission electron microscope (TEM, JEM-2010), as shown in fig. 4, it can be verified that the structure of the cathode material further indicates that the cathode material has a monodisperse nano-sheet property.
K prepared in example 22Cu0.6Zn0.4[Fe(CN)6]Carrying out electrochemical performance test: according to K2Cu0.6Zn0.4[Fe(CN)6]Weighing Super P and polyvinylidene fluoride according to the mass ratio of 7:2:1, adding a proper amount of N-methyl pyrrolidone, uniformly mixing, coating on an aluminum foil current collector, drying in vacuum at 60 ℃ for 12 hours, rolling and slicing to obtain the electrode plate. The electrode plate is used as a positive electrode, the potassium metal plate is used as a negative electrode, the microporous filter membrane is used as an isolating membrane, and 1M KPF (Ketone radical Filter) is used6The solution (dissolved in mixed solution of DEC: EC =1: 1) was used as an electrolyte, and a 2032 type button cell was assembled in a Braun glove box filled with argon gas, and a charge and discharge test was performed within a voltage range of 2.0 to 4.1V. FIG. 5 shows an embodiment2 preparation of K2Cu0.6Zn0.4[Fe(CN)6]According to the first two-time charging and discharging curves under the conditions of 2.0-4.0V and 10mA/g, the first charging specific capacity is 75.0 mAh/g, the first discharging specific capacity is 70.2 mAh/g, the first coulombic efficiency is up to 93.5%, and the high coulombic efficiency is shown. FIG. 6 shows K in example 22Cu0.6Zn0.4[Fe(CN)6]The cycle performance curve of the material under the current of 10mA/g shows that the material has better cycle stability, and the reversible discharge specific capacity retention rate of the material after 300 cycles is 79.4%.
Example 3:
the molecular formula of the nano-sheet potassium ion battery positive electrode material provided by the embodiment is K2Zn[Fe(CN)6]The preparation method comprises the following specific steps:
s1: dissolving potassium ferrocyanide in deionized water solution with the concentration of 0.5mol/L, placing the solution in an ultrasonic generating device, and taking water as a propagation medium;
s2: dissolving zinc nitrate into an ethylene glycol solution at 55 ℃, wherein the total concentration of metal ions is 0.25 mol/L;
s3: dropwise adding the mixed alcohol solution into a potassium ferrocyanide aqueous solution at the speed of 2.5 ml/h by using an injection pump, carrying out precipitation reaction, simultaneously loading ultrasonic waves with the power of 750W, replacing medium water in an ultrasonic device by using circulating water in order to adjust the reaction temperature rise caused by loading the ultrasonic waves, and controlling the reaction temperature to be about 30 ℃; the volume ratio of the final copper acetate alcohol solution to the potassium ferrocyanide aqueous solution is 1: 1.05;
s4: and washing and drying the obtained precipitate to obtain a material, thus obtaining a final finished product.
For K prepared in example 32Zn[Fe(CN)6]The material was characterized by microscopic morphology using the same equipment as in example 1. As shown in fig. 7, the nanosheet structure remained but increased in size and a small amount of nanoparticles appeared, compared to examples 1 and 2, due to the increase in ultrasonic power and the change in metal ions.
The above embodiments are described in further detail to solve the technical problems, technical solutions and advantages of the present invention, and it should be understood that the above embodiments are only examples of the present invention and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. The preparation method of the nano flaky potassium ion battery positive electrode material is characterized in that the molecular formula of the nano flaky potassium ion battery positive electrode material is K2CuxZn1-x[Fe(CN)6]Wherein x is more than or equal to 0 and less than or equal to 1, and the thickness of the lamella of the positive electrode material of the nano flaky potassium ion battery is 20-40 nm;
the method comprises the following steps:
s1: dissolving potassium ferrocyanide in a deionized water solution to obtain a solution A;
s2: dissolving soluble copper salt and soluble zinc salt in an alcohol solution, and heating and stirring to obtain a solution B;
s3: dropwise adding the solution B into the solution A, and carrying out precipitation reaction under the assistance of ultrasonic waves to obtain a precipitation product;
s4: washing and drying the precipitate to obtain the nano flaky potassium ion battery anode material;
in step S2, the soluble copper salt is any one of copper nitrate, copper sulfate, copper acetate, and copper chloride; the soluble zinc salt is any one of zinc nitrate, zinc sulfate, zinc chloride and zinc acetylacetonate; in step S2, the alcohol solution is any one of or a mixture of at least two of ethylene glycol, 1, 2-propylene glycol, and glycerol;
in step S2, the heating temperature during heating and stirring is 45-75 ℃;
in step S2, in the solution B, the total concentration of the soluble copper salt and the soluble zinc salt is 0.1-0.5 mol/L;
in the step S3, the dropping rate of the solution B is 1.0-5 ml/h;
in step S3, the ultrasonic power is 400-800W, and the frequency is 40 KHz;
in step S3, the temperature change of the reaction solution caused by the ultrasonic wave should be controlled by using circulating water, and the temperature range is 25-35 ℃;
in step S3, the volume ratio of solution A to solution B is (1.05-2): 1.
2. A potassium ion battery, characterized in that: the nano flaky potassium ion battery positive electrode material is prepared by the preparation method of claim 1.
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